CN101215462A - Method for preparing foaming agent used for oil gas field drilling and extracting - Google Patents
Method for preparing foaming agent used for oil gas field drilling and extracting Download PDFInfo
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- CN101215462A CN101215462A CNA2008100451674A CN200810045167A CN101215462A CN 101215462 A CN101215462 A CN 101215462A CN A2008100451674 A CNA2008100451674 A CN A2008100451674A CN 200810045167 A CN200810045167 A CN 200810045167A CN 101215462 A CN101215462 A CN 101215462A
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Abstract
The invention relates to a process for preparing sponging agent which is adopted by oil gas field drills and used in the drilling technology of oil and natural gas and in geothermal drilling wells. The process is the synthetic technology for improving the sponging agent, lowers the producing cost, increases the foamability and the foam stability, and is realized by two-step synthesis. The invention is characterized in that: firstly, adding epoxy chloropropane, sodium bisulfite, deionized water and alkali catalyst into a catalyst case , heating to 60-85 DEG C under mixing, reacting for 2-3 hours, processing reactants into water solution which contains 3-chlorine-2-hydroxypropyl sodium sulfonate whose concentration is 30% with the deionized water after the reactants are aged for 1hour in 70 DEG C, then, adding long-chain tertiary amine into the mixed solution of the water solution which is prepared by the above process, anionic surface active agent and water, heating to 75-95 DEG C under mixing, and reacting for 7-9 hours, preparing the sponging agent which takes N-alkyl-N and N-dimethyl hydroxypropyl sulfo betaine as main components. The reaction time of the invention is greatly shortened, the tertiary amine percent conversion is high, the surfactivity is increased, the foaming performance of the product is good, and the invention can be used for sponging agent formula which is needed in the oil field gas drills.
Description
Technical field
The present invention relates to a kind of oil and gas drilling technology and geothermal drilling of being used for, be specially adapted to contain under the fresh water or the electrolytical environment of high density of crude oil and hydrocarbon polymer, have the preparation method of the foaming agent used for oil gas field drilling and extracting of good latherability and big gun foam stability.
Background technology
Many exploitation of oil-gas field are to the middle and later periods, and payzone pressure generally descends.Simultaneously, newfound many oil-gas fields, the pressure of storage layer are not high yet, and the best method of drilling this class oil-gas field is to adopt air drilling.So-called air drilling is to utilize air, the nitrogen drilling technique as circulatory mediator.Because gas density is little, the in-hole fluid hydrostaticpressure is significantly less than conventional drilling liquid hydrostaticpressure, and it is under-voltage poor to form in the shaft bottom.So both prevented effectively that liquid and solid from entering storage layer, significantly reducing the injury to hydrocarbon zone, greatly improved rate of penetration again, therefore very promising.Because in drilling process, will run into local water inevitably and immerse pit shaft, submerged water and drilling cuttings form mud cake or agglomerate, can not be taken out of ground by gas effectively, seriously disturb carrying out smoothly of drilling well.Whipping agent can disperse drilling tool adherent landwaste and mud cake effectively, fully disperses stratum submerged liquid, and the act of enhance fluid bits ability makes the mineshaft annulus inner fluid be steady state greatly; Whipping agent is the Castor Oil drilling tool and the borehole wall also, forms protective membrane at the borehole wall, reduces the erosion of fluid to the borehole wall, improves bore hole borehole wall quality, reduces the frictional resistance loss.Therefore, whipping agent is the smooth important assurance of air drilling.
In the natural-gas field recovery process, watered-out well occurring is ubiquitous problem.The best approach that solves is a foaming water discharge.Promptly inject whipping agent in the gasser that hydrops is arranged, Sweet natural gas, hydrops and whipping agent form foam at the shaft bottom thorough mixing, and density reduces greatly, and foam can reduce the slippage of water simultaneously, improve the air-flow fluid-carrying capability, reduce the shaft bottom back pressure, increase gas output.This technology construction is easy, less investment, and cost is low, and instant effect does not influence the gas well ordinary production, thereby extensively is used.
Foam also can be used for technologies such as well cementing of cement, sand-flushing, profile control, pressure break, acidifying, so whipping agent has purposes widely in natural petroleum gas field industry.But in above-mentioned employing foamy technology, foam all will contact with local water with the stratum, this foam that just requires to produce is containing the some amount soluble salt, in the water as sodium-chlor, calcium chloride, magnesium chloride etc. high froth stability is arranged, to influencing some factors of foam stabilization, as crude oil, solia particle higher tolerance is arranged, but also must under extreme physical environment such as high temperature, highly compressed situation, not degrade.Also require under strong acid and high density ionogen existing good froth stability also not degrade to the acidifying foam.
Summary of the invention
The objective of the invention is: in order to improve the synthesis technique of N-alkyl-N-N-dimethyl hydroxypropyl sultaine, reduce production costs, increase substantially it in fresh water and the water or latherability in the strong acid and the froth stability that contain ionogen or hydrocarbon polymer, at high temperature do not degrade the special preparation method who proposes a kind of foaming agent used for oil gas field drilling and extracting.
Principle of the present invention is at synthetic amphoterics N-alkyl-N, during N-dimethyl hydroxypropyl sultaine, adds a kind of anion surfactant, not only can improve reaction conditions, shortens the reaction times, improves transformation efficiency.Simultaneously, can obtain the good whipping agent of foaming properties.This whipping agent has improved the resistivity of hydro carbons to the foam infringement greatly, is still keeping good foaming properties in electrolytical environment such as soluble inorganic salt, strong acid, its details describe as after.
N-alkyl-N, N-dimethyl hydroxypropyl sultaine, molecular formula RN (CH
3)
2CH
2CH (OH) CH
2SO
3 -(R is the straight or branched alkyl of carbonatoms 8-18) is a kind of amphoterics.Its surfactivity is strong, and foam is abundant, and the salt dissolubility is good, and is stable in soda acid, has good anti-hard water and dispersion of calcium soap, of many uses.
N-alkyl-N, N-dimethyl hydroxypropyl sultaine has multiple synthetic route
[1], wherein two lines are better synthetic.The first is then handled tertiary amine and epoxy chloropropane effect with S-WAT, the result mainly obtains the mixture of two kinds of hydroxypropyl sulfonation trimethyl-glycines
RN
+(CH
3)
2CH
2CHOHCH
2SO
3 -And RN
+(CH
3)
2CH (CHOH) CH
2SO
3 -
Obviously, this is not a kind of best synthetic route; It two is that S-WAT and epichlorohydrin reaction are prepared 3-chloro-2-hydroxypropionate sodium ClCH
2CH (OH) CH
2SO
3Na is again with long chain tertiary amine RN (CH
3)
2, (the R=C atomicity is the straight or branched alkyl of 8-18), with the effect of 3-chloro-2-hydroxypropionate sodium, the compound R N that obtains determining
+(CH
3)
2CH
2CHOHCH
2SO
3 -Its reaction is as follows
In actual production, all adopt a kind of route in back.In this synthetic route, long chain tertiary amine and 3-chloro-2-hydroxypropyl azochlorosulfonate acid sodium act as inhomogeneous reaction, in order to shorten the reaction times, improve the tertiary amine transformation efficiency, all in the aqueous solution of single or polyhydroxy-alcohol such as ethanol, glycerol, carry out during production.Nonetheless, the time of reaction is also quite long, reaches more than 30 hour sometimes.Remaining tertiary amine does not have surfactivity.
The present invention finds that with the synthetic N-alkyl-N of this route, in the process of N-dimethyl hydroxypropyl sultaine tensio-active agent, adding a kind of molecular formula is R
1O (CH
2CH
2O) n (CH
2) mCH (X) CH
2YM, (R
1=C atomicity is the saturated or undersaturated straight or branched alkyl of 8-22, n=0-6, m=1-3, X=-H ,-OH or-CH
3, Y is-COO
-Or-SO
3 -, M=Na, K, NH
4Deng) anion surfactant, can make building-up reactions in water, carry out (need not add alcohol), the reaction times shortens greatly, the tertiary amine transformation efficiency improves, and the foaming properties of product is good.
In order to achieve the above object, the technical solution used in the present invention is: a kind of preparation method of foaming agent used for oil gas field drilling and extracting, synthesize and realize by two steps, its technical characterictic is: the first step, synthesizing of 3-chloro-2-hydroxypropyl azochlorosulfonate acid sodium (representing) with II, be reflected in the container of sealing and carry out, earlier with epoxy chloropropane 1.0mol, sodium bisulfite 1.05mol, deionized water 280-300ml, alkaline catalysts 0.1g-1.0g joins in the reactor, under agitation be heated to 60-85 ℃, reaction 2-3h, reactant is processed into the aqueous solution that contains 3-chloro-2-hydroxypropyl azochlorosulfonate acid sodium 30% concentration with deionized water behind 70 ℃ of ageing 1h; Second step, N-alkyl-N, N-dimethyl hydroxypropyl sultaine (representing with I) synthetic is with long chain tertiary amine RN (CH
3)
2(representing with III) is added in the mixing solutions of 3-chloro-2-hydroxypropyl azochlorosulfonate acid sodium (II) aqueous solution that obtains with aforesaid method and anion surfactant (representing with IV) and water, their weight ratio is, III: II: IV: water=100: 90-110: 1-50: 200-400, the aqueous solution that maybe will contain 3-chloro-2-hydroxypropyl azochlorosulfonate acid sodium (II) is added in the mixing solutions of III and IV and water, their weight ratio is, II: III: IV: water=90-110: 100: 1-50: 200-400, under agitation be heated to 75-95 ℃, reacted 7-9 hour, make alkyl-N with N-, N-dimethyl hydroxypropyl sultaine is the whipping agent of main component.The catalyzer that subtracts of the present invention is NaOH, Ca (OH)
2, Na
2CO
3/ in a kind of.The described anion surfactant of this law is that molecular formula is R
1O (CH
2CH
2O) n (CH
2) mCHOHCH
2COONa (K), R
1O (CH
2CH
2O) n (CH
2) mCH
2CH
2COONa (K), R
1O (CH
2CH
2O) n (CH
2) mCH
2CH
2SO
3Na (K), R
1O (CH
2CH
2O) n (CH
2) mCHOHCH
2SO
3Na (K), R
1O (CH
2CH
2O) n (CH
2) mCHCH
3CH
2COONa (K), R
1O (CH
2CH
2O) n (CH
2) mCHCH
3CH
2SO
3A kind of (R in the formula of Na (K)
1=C atomicity is the saturated or undersaturated straight or branched alkyl of 8-22, n=0-6, and m=1-3), the described long chain tertiary amine of this law is C
8H
17N (CH
3)
2, C
10H
21N (CH
3)
2, C
12H
25N (CH
3)
2, C
14H
29N (CH
3)
2, C
16H
33N (CH
3)
2In a kind of or their mixture.The described reaction of this law must be carried out in basic solution, and the pH value of control solution is in the scope of 7.5-8.5 in the entire reaction course.
The invention has the beneficial effects as follows: (1) synthesizes N-alkyl-N, and N-dimethyl hydroxypropyl sultaine does not need to carry out in alcoholic solution, and the reaction times shortens greatly, tertiary amine transformation efficiency height; (2) because the product of reaction is single, tertiary amine transformation efficiency height, residual tertiary amine (no surfactivity) and 3-chloro-2-hydroxypropyl azochlorosulfonate acid sodium are all seldom, N-alkyl-N that anion surfactant (IV) and reaction simultaneously generates, N-dimethyl hydroxypropyl sultaine (I) has very strong synergy, improved the surfactivity of product greatly, foaming properties is all better than original component.And good complex role is arranged with other tensio-active agents, can obtain being applicable to that the exploitation of oil-gas field difference requires needed whipping agent prescription.
Embodiment
The test result of this working of an invention method and product performance is described below in conjunction with technical scheme of the present invention:
Example 1. adds 27.5% sodium sulfite solution 415 grams in 1 liter of reactor, add 10%NaOH solution 1ml, put the reaction kettle cover, under agitation be warmed to 65 ℃, then add epoxy chloropropane 100 grams, 65-75 ℃ of reaction 2.5 hours, reactant was 70 ℃ of ageings 1 hour, add water 190ml, get 30% 3-chloro-2-hydroxypropyl azochlorosulfonate acid sodium solution 706 grams.
In the 1000ml there-necked flask, 3-chloro-2-hydroxypropyl azochlorosulfonate acid sodium solution 330 grams of adding 30%, deionized water 120ml, add anion surfactant (IV) 50 grams again, be heated to 75 ℃, under this temperature, stirred 30 minutes, add dodecyl dimethyl amine 100 grams, with the phenolphthalein agent of giving instruction, drip 10% NaOH solution, the pH value of control reaction system is at 7.5-8.5, continuation was 75-95 ℃ of reaction 8 hours, obtain the yellow little band heavy-gravity liquid of little band, measure its unhindered amina value, the transformation efficiency of tertiary amine 〉=99.5%.
Example 2. adds 100 gram C in the 1000ml there-necked flask
12-14Dimethyl tertiary amine, 190ml deionized water, 30 gram anion surfactants (IV) add 30% 3-chloro-2-hydroxypropyl azochlorosulfonate acid sodium solution 300 grams of example 1 preparation again, are heated to 85 ℃, stir 1 hour.Make indicator with phenolphthalein, drip 15% NaOH solution, the pH value of control reaction system keeps 75-95 ℃ to continue reaction 8h at 7.5-8.5, obtains than thick liquid, measures its residual tertiary amine≤0.5%
The test of example 3. foaming properties.Here adopt Waring Blender paddling process to test the foaming properties of whipping agent under different condition.The american petroleum industrial sector often adopts this method, and China Petroleum department also adopts this method usually.Used instrument is the Waring-Blender agitator, during test, adds the 100ml test fluid at graduated jar, at a high speed (〉=5000rpm) stir 60s after, close switch, write down lather volume (V) immediately, represent the latherability of whipping agent with this, V is big more, and latherability is strong more.Write down immediately and from foam, separate out the needed time of 50ml liquid (t), be called foamy (discharge opeing) transformation period, reflection foamy stability, t is long more, and foam is stable more.Latherability and froth stability are the topmost performances of whipping agent, and therefore, the numeric ratio of V and t is expressed the character of whipping agent preferably.
Table 1 has been listed this whipping agent (X that synthesizes by example 1
1) and DSB (N-dodecyl-N, N-dimethyl hydroxypropyl sultaine), anion surfactant IV and oil-gas field whipping agent SDS (sodium lauryl sulphate), AES (alkyl polyoxyethylene ether sodium sulfate), ABS (sodium alkyl benzene sulfonate), the foaming properties of BS-12 (alkyl betaine) under the different quality condition commonly used.
Table 1
| Tap water | 10% (v/v) crude oil | 10％NaCl | 1％CaCl 2+ 4%NaCl+10% crude oil (v/v) | |||||
| V(ml) | t(m:s) | V(ml) | t(m:s) | V(ml) | t(m:s) | V(ml) | t(m:s) | |
| SDS AES ABS BS-12 DSB IV X 1 | 450 285 330 495 390 430 580 | 4:38 2:23 2:54 3:45 2:37 2:37 9:39 | 400 150 285 180 160 525 623 | 5:16 1:15 3:18 5:09 1:05 7:12 11:07 | 475 260 155 500 305 500 595 | 4:15 3:15 1:44 3:37 2:17 6:25 10:19 | 145 150 still 140 120 130 450 | 0:48 0:39 0:21 0:19 0:42 2:19 |
Annotate: surfactant concentrations is 0.25%
Several tensio-active agents of listing, X under different condition
1Foaming properties best.At CaCl
2, the coexistence of NaCl and crude oil system in, the foaming properties of tensio-active agent is all very poor, X
1V and t also descend more, but X
1Foaming properties can add a small amount of ethylene glycol or derivatives thereof and improve greatly, see Table 2.
Table 2
| Add 10% crude oil (v/v) | Add 15% crude oil (v/v) | |||
| V(ml) | t(m:s) | V(ml) | t(m:s) | |
| X 10.25%, ethylene glycol 0.12%, NaCl 4%, CaCl 2 1％ | 570 | 8:58 | 595 | 12:04 |
Therefore, in the actual use of oil-gas field, when running into the situation of the local water that contains bittern and oil coexistence, at X
1The a small amount of ethylene glycol or derivatives thereof of middle adding is a well prescription, and its proportional quantity is determined by circumstances.
Sodium lauryl sulphate (SDS), alkyl polyoxyethylene ether sodium sulfate (AES) are unstable in strong acid, easily decompose; Sodium dodecylbenzene sulfonate (ABS) generates precipitation in calcium salt non-foaming; Alkyl betaine (BS-12) is an amphoterics, and iso-electric point is arranged, and X
1Good foaming properties is all arranged in strong electrolyte solution such as hydrochloric acid, calcium chloride, see Table 3
N-dodecyl-N, N-dimethyl hydroxypropyl sultaine, though be a kind of amphoterics, it does not have iso-electric point.
Table 3
| HCl concentration (%) | V(ml) | t(m:s) | CaCl 2Concentration (%) | V(ml) | t(m:s) |
| 6 9 15 24 | 630 580 545 500 | 8:33 8:02 8:02 11:05 | 5 10 20 30 | 588 570 490 475 | 9:22 10:30 10:49 12:18 |
Therefore, X
1Can be used as the whipping agent of foamed acid metallization processes.
X
1The thermally-stabilised height of tensio-active agent has the good heat-resistance decomposability, and 200 ℃ of insulations 12 hours, foaming properties did not have much variations before and after the heating, sees Table 4 with its aqueous solution of 0.25%
Table 4
| Foaming properties before the heating | Heating back foaming properties | ||
| V(ml) | t(m:s) | V(ml) | t(m:s) |
| 580 | 9:23 | 585 | 9:20 |
In high temperature operations such as the displacement of reservoir oil of high temperature reservoir, deep-well water pumping gas production, geothermal drilling, all need the high whipping agent of thermostability.
Claims (5)
1. the preparation method of a foaming agent used for oil gas field drilling and extracting is to be synthesized by two steps to realize, it is characterized in that: the first step, be reflected in the container of sealing and carry out, first with epoxy chloropropane 1.0mol, sodium bisulfite 1.05mol, deionized water 280-300ml, alkaline catalysts 0.1-1.0g, join in the reactor, under agitation be heated to 60-85 ℃, reaction 2-3h, reactant is processed into the aqueous solution that contains 3-chloro-2-hydroxypropyl azochlorosulfonate acid sodium 30% concentration with deionized water behind 70 ℃ of ageing 1h; Second step, again with long chain tertiary amine, join in the mixing solutions of 3-chloro-2-hydroxypropyl azochlorosulfonate acid sodium solution that aforesaid method makes and anion surfactant and water, their weight ratio is: tertiary amine: 3-chloro-2-hydroxypropyl azochlorosulfonate acid sodium: anion surfactant: water=100: 90-100: 1-50: 200-400, the solution that maybe will contain 3-chloro-2-hydroxypropyl azochlorosulfonate acid sodium joins in the mixing solutions of long chain tertiary amine and anion surfactant and water, their weight ratio is: 3-chloro-2-hydroxypropyl azochlorosulfonate acid sodium: long chain tertiary amine: anion surfactant: water=90-110: 100: 1-50: 200-400, under agitation be heated to 75-95 ℃, reaction 7-9h, make N-alkyl-N, N-dimethyl hydroxypropyl sultaine.
2. according to the preparation method of the described whipping agent of claim 1, it is characterized in that: the described catalyzer that subtracts of this law is with NaOH, Ca (OH)
2, Na
2CO
3A kind of.
3. according to the preparation method of the described whipping agent of claim 1, it is characterized in that: the described long chain tertiary amine of this law is to use C
8H
17N (CH
3)
2, C
10H
21N (CH
3)
2, C
12H
25N (CH
3)
2, C
14H
29N (CH
3)
2, C
16H
33N (CH
3)
2In a kind of or their mixture.
4. according to the preparation method of the described whipping agent of claim 1, it is characterized in that: the described anion surfactant of this law is to use R
1O (CH
2CH
2O) n (CH
2) mCHOHCH
2COONa (K), R
1O (CH
2CH
2O) n (CH
2) mCH
2CH
2COONa (K), R
1O (CH
2CH
2O) n (CH
2) mCH
2CH
2SO
3Na (K), R
1O (CH
2CH
2O) n (CH
2) mCHOHCH
2SO
3Na (K), R
1O (CH
2CH
2O) n (CH
2) mCHCH
3CH
2COONa (NH
4), R
1O (CH
2CH
2O) n (CH
2) mCHCH
3CH
2SO
3Na (NH
4) a kind of, R in the formula
1=C atomicity is the saturated or undersaturated straight or branched alkyl of 8-22, n=0-6, m=1-3.
5. according to the preparation method of the described whipping agent of claim 1, it is characterized in that: the described reaction of this law must be carried out in basic solution, and the pH value of control solution is in the scope of 7.5-8.5 in the entire reaction course.
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|---|---|---|---|
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